CN113302321A - Method for producing unidirectional electromagnetic steel sheet - Google Patents

Method for producing unidirectional electromagnetic steel sheet Download PDF

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Publication number
CN113302321A
CN113302321A CN202080009242.0A CN202080009242A CN113302321A CN 113302321 A CN113302321 A CN 113302321A CN 202080009242 A CN202080009242 A CN 202080009242A CN 113302321 A CN113302321 A CN 113302321A
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steel sheet
annealing
rolled steel
hot
cold
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安田雅人
高桥克
牛神义行
长野翔二
财前洋一
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Nippon Steel Corp
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Nippon Steel and Sumitomo Metal Corp
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Abstract

The method for producing a unidirectional electromagnetic steel sheet of the present invention comprises: heating a billet having a predetermined chemical composition to less than 1250 ℃ and subjecting the billet to hot rolling to form a hot-rolled steel sheet, subjecting the hot-rolled steel sheet to hot-rolled sheet annealing, subjecting the hot-rolled steel sheet after the hot-rolled sheet annealing to acid pickling, subjecting the hot-rolled steel sheet after the acid pickling to cold rolling to form a cold-rolled steel sheet having a final thickness d of 0.15 to 0.23mm, subjecting the cold-rolled steel sheet to decarburization nitriding treatment including decarburization annealing and nitriding treatment, subjecting the cold-rolled steel sheet after the decarburization nitriding treatment to finish annealing, and applying an insulating film-forming coating liquid to the cold-rolled steel sheet after the finish annealing and sintering the coating liquid; wherein Sol.Al/N, which is a mass ratio of Sol.Al to N, of the billet and the final sheet thickness d satisfy a predetermined relational expression, the N content of the cold-rolled steel sheet after the decarburization nitriding treatment is 40 to 1000ppm, and the decarburization annealing temperature in the decarburization annealing is lower than 1000 ℃.

Description

Method for producing unidirectional electromagnetic steel sheet
Technical Field
The present invention relates to a method for producing a grain-oriented electrical steel sheet.
The present application claims priority based on application No. 2019-005202 filed in japan on day 16/01/2019, the contents of which are incorporated herein by reference.
Background
The grain-oriented electrical steel sheet is a soft magnetic material and is used for iron cores of transformers (transformers) and other electrical devices. A unidirectional electromagnetic steel sheet contains about 7 mass% or less of Si and has crystal grains highly concentrated in the {110} <001> orientation in terms of Miller index.
For the magnetic properties of the grain-oriented electrical steel sheet used for the above-mentioned applications, it is required that the magnetic flux density (represented by the value of B8 when a magnetic field of 800A/m is applied) is high and the iron loss (the energy loss W when the magnetization is carried out at a maximum magnetic flux density of 1.7T in an alternating current at a frequency of 50 Hz)17/50Representative) is low. In particular, recently, from the viewpoint of energy saving, there is an increasing demand for reduction of power loss.
The iron loss of an electrical steel sheet is determined by the sum of eddy current loss depending on resistivity, sheet thickness, magnetic domain size, and the like, and hysteresis loss depending on crystal orientation, surface smoothness, and the like. Therefore, to reduce the iron loss, it is necessary to reduce one or both of the eddy current loss and the hysteresis loss.
As a method for reducing eddy current loss, a method of increasing the content of Si having high electric resistance, a method of reducing the thickness of a steel sheet, a method of refining magnetic domains, and the like are known. As a method for reducing hysteresis loss, a method of increasing the magnetic flux density B8 by increasing the concentration of easy magnetization orientation of crystal orientation, and a method of removing a pinning effect that inhibits magnetic domain movement by smoothing a glass coating formed of an oxide on the surface of a steel sheet are known.
Among these methods for reducing the iron loss, as a method for smoothing the surface of a steel sheet, for example, patent documents 1 to 5 disclose that an Fe-based oxide (Fe) is not generated2SiO4FeO, etc.) and an annealing separating agent mainly composed of alumina is used as an annealing separating agent interposed between steel plates, and a glass coating (forsterite coating) is not formed.
As a method for reducing the thickness of a steel sheet, a method for reducing the thickness by rolling is known, but if the thickness is reduced, secondary recrystallization in finish annealing becomes unstable, and there is a problem that it is difficult to stably produce a product excellent in magnetic properties.
In view of the above problem, for example, patent document 6 proposes a method for manufacturing a unidirectional electromagnetic steel sheet in which a cold-rolled steel sheet having a thickness dmm of 0.10 to 0.25mm is subjected to decarburization annealing and nitriding treatment and AlN is used as a suppressor, wherein the suppressor is strengthened by setting acid-soluble Al to 0.015 to 0.050% and by nitriding so that the nitrogen content [ N ] of the steel sheet is 13 d-25 ≧ [ N ] > 46 d-1030, thereby stably manufacturing a thin unidirectional electromagnetic steel sheet.
However, the method of patent document 6 has a problem that the film properties are poor because a large amount of nitrogen is released after the glass film is formed.
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. H07-118750
Patent document 2: japanese laid-open patent publication No. H07-278668
Patent document 3: japanese laid-open patent publication No. H07-278669
Patent document 4: japanese patent laid-open publication No. 2003-003213
Patent document 5: japanese patent publication No. 2011-518253
Patent document 6: japanese laid-open patent publication No. H05-302122
Disclosure of Invention
Problems to be solved by the invention
It is assumed that the problems of the method of patent document 6 can be solved by introducing a method of smoothing the surface of a steel sheet without forming a glass film (forsterite film) as shown in patent documents 1 to 5, but in the method of smoothing the surface of a steel sheet, it is difficult to ensure good decarburization and decarburization is inferior with an increase in Al content. Therefore, in a thin electrical steel sheet, if the Al content is increased in order to stably obtain a secondary recrystallized structure, it is difficult to achieve both decarburization properties and to obtain excellent magnetic properties.
Accordingly, an object of the present invention is to provide a method for manufacturing a grain-oriented electrical steel sheet, which solves the problem of stably obtaining a good secondary recrystallized structure, by reducing the sheet thickness of a grain-oriented electrical steel sheet containing a desired amount of Al to reduce the iron loss and by ensuring good decarburization to improve the magnetic properties (to reduce the iron loss and to ensure a high magnetic flux density).
Means for solving the problems
In order to solve the above problems, the present inventors investigated the relationship between the Al content and the sheet thickness in order to stably obtain secondary recrystallization and ensure good decarburization performance in a thin grain-oriented electrical steel sheet produced by a method of smoothing the surface of the steel sheet.
As a result, it was found that: the mass ratio of acid-soluble Al (sol. Al) to N in the billet as a raw material is determined by the product thickness, that is, the final thickness d after cold rolling: al/N is controlled to an appropriate range, so that good decarburization can be ensured in decarburization annealing, and good secondary recrystallization can be obtained in finish annealing by controlling the N content of the steel sheet subjected to nitriding to an appropriate range. This point will be described later.
The present invention has been completed based on the above findings, and the gist thereof is as follows.
(1) A method for manufacturing a grain-oriented electrical steel sheet according to an aspect of the present invention includes: heating a steel slab to less than 1250 ℃ and subjecting to hot rolling to form a hot-rolled steel sheet, the steel slab containing, in mass%, C: 0.100% or less, Si: 0.80 to 7.00%, Mn: 0.05-1.00%, Sol.Al: 0.0100-0.0700%, N: 0.0040-0.0120%, Seq ═ S +0.406 × Se: 0.0030-0.0150%, Cr: 0-0.30%, Cu: 0-0.40%, Sn: 0-0.30%, Sb: 0-0.30%, P: 0-0.50%, B: 0-0.0080%, Bi: 0-0.0100%, Ni: 0 to 1.00% and the balance containing Fe and impurities, subjecting the hot-rolled steel sheet to hot-rolled sheet annealing, subjecting the hot-rolled steel sheet after the hot-rolled sheet annealing to acid pickling, subjecting the hot-rolled steel sheet after the acid pickling to cold rolling to form a cold-rolled steel sheet having a final thickness d of 0.15 to 0.23mm, subjecting the cold-rolled steel sheet to decarburization nitriding treatment including decarburization annealing and nitriding treatment, subjecting the cold-rolled steel sheet after the decarburization nitriding treatment to finish annealing, and applying an insulating film-forming coating liquid to the cold-rolled steel sheet after the finish annealing and sintering the coating liquid; wherein Sol.Al/N, which is a mass ratio of Sol.Al to N, of the billet and the final plate thickness d satisfy the following formula (i), the N content of the cold-rolled steel sheet after the decarburization nitriding treatment is 40 to 1000ppm, and the decarburization annealing temperature in the decarburization annealing is lower than 1000 ℃.
－4.17×d+3.63≤Sol.Al/N≤－3.10×d+4.84 (i)
(2) The method for producing a grain-oriented electrical steel sheet according to the item (1), wherein the slab may contain, in mass%, Cr: 0.02 to 0.30%, Cu: 0.10 to 0.40%, Sn: 0.02 to 0.30%, Sb: 0.02-0.30%, P: 0.02-0.50%, B: 0.0010 to 0.0080%, Bi: 0.0005 to 0.0100%, Ni: 0.02-1.00% of 1 or more.
Effects of the invention
The present invention can provide a method for stably producing a grain-oriented electrical steel sheet having a sheet thickness of 0.15 to 0.23mm and excellent magnetic properties (low iron loss and high magnetic flux density).
Drawings
FIG. 1 shows an example of the structure of a grain-oriented electrical steel sheet obtained by a manufacturing method in which the slab heating temperature is 1250 ℃ and the decarburization annealing temperature is 800 ℃.
FIG. 2 shows an example of the structure of a grain-oriented electrical steel sheet obtained by a manufacturing method in which the slab heating temperature is 1150 ℃ and the decarburization annealing temperature is 800 ℃.
Detailed Description
A method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention (hereinafter, sometimes referred to as "manufacturing method according to the present embodiment") includes: heating a steel slab to less than 1250 ℃ and subjecting to hot rolling to form a hot-rolled steel sheet, the steel slab containing, in mass%, C: 0.100% or less, Si: 0.80 to 7.00%, Mn: 0.05-1.00%, Sol.Al: 0.0100-0.0700%, N: 0.0040-0.0120%, Seq ═ S +0.406 × Se: 0.0030-0.0150%, Cr: 0-0.30%, Cu: 0-0.40%, Sn: 0-0.30%, Sb: 0-0.30%, P: 0-0.50%, B: 0-0.0080%, Bi: 0-0.0100%, Ni: 0 to 1.00% and the balance containing Fe and impurities, subjecting the hot-rolled steel sheet to hot-rolled sheet annealing, pickling, and cold-rolling to form a cold-rolled steel sheet having a final thickness of 0.15 to 0.23mm, subjecting the cold-rolled steel sheet to decarburization nitriding including decarburization annealing and nitriding, and then performing finish annealing, and applying an insulating film-forming coating liquid to the cold-rolled steel sheet after the finish annealing and sintering (also referred to as "burning"); the manufacturing method is characterized in that:
(i) mass ratio of acid-soluble Al (sol. Al) to N of the billet: sol. Al/N and the final plate thickness d (mm) satisfy the following formula (1);
(ii) the N content of the cold-rolled steel sheet subjected to decarburization and nitridation treatment is 40-1000 ppm; and is
(iii) The decarburization annealing temperature in the decarburization annealing is lower than 1000 ℃.
－4.17×d+3.63≤Sol.Al/N≤－3.10×d+4.84 (1)
The following describes a manufacturing method according to the present embodiment. The manufacturing method according to the present embodiment is preferably used as a method for manufacturing a grain-oriented electrical steel sheet having no forsterite coating, but can exhibit significant effects even when used as a method for manufacturing a grain-oriented electrical steel sheet having a forsterite coating.
First, the reason why the composition of the billet as a raw material is limited in the manufacturing method according to the present embodiment will be described. Hereinafter,% means mass%.
< composition of ingredients >
C: less than 0.100%
C is an element effective for controlling the primary recrystallization structure, but is an element to be removed by decarburization annealing before finish annealing because it adversely affects the magnetic properties. If the C content in the steel slab exceeds 0.100%, the decarburization annealing time is prolonged and the productivity is lowered. Therefore, the C content is set to 0.100% or less. The C content is preferably 0.070% or less, more preferably 0.060% or less.
The lower limit of the C content includes 0%, but if the C content is reduced to less than 0.0001%, the manufacturing cost is greatly increased, and 0.0001% is a substantial lower limit of the C content in a practical steel sheet. The lower limit of the C content may be set to 0.0010%, 0.0020%, 0.0022%, or 0.0030%.
Si：0.80～7.00％
Si is an element that increases the electrical resistance of the steel sheet and improves the iron loss characteristics of the grain-oriented electrical steel sheet. If the Si content is less than 0.80%, γ transformation occurs during finish annealing, which impairs the aggregation of the preferred crystal orientation of the steel sheet, so the Si content is set to 0.80% or more. The Si content is preferably 1.80% or more, 1.90% or more, 2.00% or more, and more preferably 2.50% or more.
On the other hand, if the Si content exceeds 7.00%, workability is deteriorated and cracks occur during rolling. Therefore, the Si content is set to 7.00% or less. The Si content is preferably 4.50% or less, more preferably 4.00% or less.
Mn：0.05～1.00％
Mn is an element that can prevent cracking during hot rolling and forms MnS and/or MnSe that function as an inhibitor by binding to S and/or Se. When the Mn content is less than 0.05%, the effect cannot be sufficiently exhibited, so the Mn content is set to 0.05% or more. The Mn content is preferably 0.07% or more, and more preferably 0.09% or more.
On the other hand, if the Mn content exceeds 1.00%, precipitation dispersion of MnS and/or MnSe becomes uneven, a desired secondary recrystallized structure is not obtained, and the magnetic flux density is lowered. Therefore, the Mn content is set to 1.00% or less. The Mn content is preferably 0.80% or less, more preferably 0.60% or less or 0.55% or less.
Acid soluble Al (sol. Al): 0.0100-0.0700%
Al (sol. Al) is an element that forms (Al, Si) N functioning as an inhibitor by bonding with N. When the sol.al content is less than 0.0100%, the effect cannot be sufficiently exhibited, and the secondary recrystallization cannot be sufficiently performed, so the sol.al content is set to 0.0100% or more. The sol-al content is preferably 0.0150% or more, more preferably 0.0200% or 0.0220% or more.
On the other hand, if the sol.al content exceeds 0.0700%, the precipitation dispersion of (Al, Si) N becomes uneven, the desired secondary recrystallized structure cannot be obtained, and the magnetic flux density decreases. Therefore, the acid-soluble Al (sol. Al) content is set to 0.0700% or less. The sol.al content is preferably 0.0550% or less, more preferably 0.0500% or less or 0.0400% or less.
N：0.0040～0.0120％
N is an element that forms AlN functioning as an inhibitor by bonding with Al, but is also an element that forms bubbles (voids) in the steel sheet at the time of cold rolling. If the N content is less than 0.0040%, AlN formation becomes insufficient, so the N content is set to 0.0040% or more. The N content is preferably 0.0050% or more or 0.0060% or more, and more preferably 0.0070% or more.
On the other hand, if the N content exceeds 0.0120%, bubbles (voids) may be formed in the steel sheet during cold rolling, so the N content is set to 0.0120% or less. The N content is preferably 0.0100% or less, more preferably 0.0090% or less.
Seq＝S+0.406×Se：0.0030～0.0150％
S and Se are elements that form MnS and/or MnSe that function as inhibitors by binding to Mn. The total content of S and Se is defined as Seq +0.406 × Se in consideration of the atomic weight ratio of S and Se.
If the Seq is less than 0.0030%, the effect cannot be sufficiently exhibited, and therefore, the Seq is set to 0.0030% or more. The Seq is preferably 0.0050% or more, more preferably 0.0070% or more. On the other hand, if the Seq exceeds 0.0150%, the precipitation dispersion of MnS and/or MnSe becomes non-uniform, the desired secondary recrystallized structure cannot be obtained, and the magnetic flux density decreases. Therefore, Seq was set to 0.0150%. The Seq is preferably 0.0130% or less, and more preferably 0.0110% or less.
In the manufacturing method according to the present embodiment, the remainder excluding the above elements in the chemical components of the billet as the raw material is Fe and impurities, but the steel sheet may contain Cr: 0.30% or less, Cu: 0.40% or less, Sn: 0.30% or less, Sb: 0.30% or less, P: 0.50% or less, B: 0.0080% or less, Bi: 0.0100% or less and Ni: 1.00% or less, or 1 or more. However, even if the billet does not contain these components, the production method according to the present embodiment can provide excellent effects. Therefore, the lower limit of the content of these components is 0%.
Cr：0～0.30％
Cr is an element contributing to an improvement in an oxide layer formed during decarburization annealing of a steel sheet, an increase in the inherent resistance of the steel sheet, and a reduction in iron loss. Since the effect is saturated if the Cr content exceeds 0.30%, the Cr content is set to 0.30% or less. The Cr content is preferably 0.25% or less. The lower limit of the Cr content is 0% or more, but is preferably 0.02% or more in view of surely obtaining the effect of containing Cr.
Cu：0～0.40％
Cu is an element that forms precipitates functioning as an inhibitor by binding to S and/or Se, and contributes to improvement of the inherent resistance of the steel sheet and the magnetic properties. In order to obtain this effect, the Cu content is preferably set to 0.10% or more.
On the other hand, if the Cu content exceeds 0.40%, the effect of reducing the iron loss is saturated because the precipitates are unevenly dispersed, so that the Cu content is set to 0.40% or less. The Cu content is preferably 0.25% or less.
Sn：0～0.30％
Sb：0～0.30％
Sn and Sb are elements that have the functions of increasing the intrinsic resistance, contributing to the reduction of the iron loss, and segregating into grain boundaries, and preventing Al from being oxidized by moisture released from the annealing separator during the annealing of the finished product (the concentration of the gaussian orientation of the texture varies due to the difference in strength of the inhibitor at the coil position, and the magnetic properties of the Al fluctuate).
If the content of any of Sn and Sb exceeds 0.30%, the effect of its inclusion is saturated, so that any of the Sn content and Sb content is set to 0.30% or less. It is preferable that any element is 0.25% or less. The lower limits of the Sn content and the Sb content include 0%, but in order to obtain the effects thereof, it is preferable that any element is 0.02% or more.
P：0～0.50％
P is an element for improving the Gaussian orientation concentration of the texture and the inherent resistance of the steel plate, and is helpful for reducing the iron loss. If the P content exceeds 0.50%, the effect is saturated and the rolling property is reduced, so that the P content is set to 0.50% or less. The P content is preferably 0.35% or less. The lower limit of the P content is 0% or more, but is preferably 0.02% or more in terms of surely obtaining the effect.
B：0～0.0080％
B is an element which combines with N to precipitate in a composite form with MnS or MnSe to form BN functioning as an inhibitor, thereby increasing the Gaussian orientation concentration of the texture and contributing to the reduction of the iron loss. In order to obtain this effect, the content of B is preferably set to 0.0010% or more.
On the other hand, if the B content exceeds 0.0080%, the precipitation dispersion of BN becomes non-uniform, the desired secondary recrystallized structure is not obtained, and the magnetic flux density is lowered. Therefore, the B content is set to 0.0080% or less. The B content is preferably 0.0060% or less, more preferably 0.0040% or less.
Bi：0～0.0100％
Bi is an element that stabilizes precipitates such as sulfides, strengthens the function of an inhibitor, increases the Gaussian orientation aggregation of a texture, and contributes to the reduction of iron loss. Since the effect is saturated if the Bi content exceeds 0.0100%, the Bi content is set to 0.0100% or less. The Bi content is preferably 0.0070% or less. The lower limit of the Bi content is 0%, but the Bi content is preferably 0.0005% or more in view of surely obtaining the effect of the Bi content.
Ni：0～1.00％
Ni is an element that contributes to an increase in the inherent resistance of the steel sheet, a reduction in the iron loss, and an improvement in the magnetic properties by controlling the metal structure of the hot-rolled steel sheet. If the Ni content exceeds 1.00%, the secondary recrystallization cannot be stably performed, so the Ni content is set to 1.00% or less. The Ni content is preferably 0.25% or less. The lower limit of the Ni content includes 0%, but the Ni content is preferably 0.02% or more in order to surely obtain the effect of containing Ni.
In the manufacturing method according to the present embodiment, the billet as a raw material contains Fe and impurities as the remainder other than the above elements. The impurities are elements mixed from a steel material and/or in a steel-making process, and are elements that can be tolerated within a range that does not impair the characteristics of the electrical steel sheet. For example, it is permissible to contain Mg, Ca, and the like in a range that does not impair the properties of the electrical steel sheet.
Next, for the mass ratio of acid-soluble Al (sol. Al) to N (ratio of content in mass%): the relationship between Al/N and the final thickness d of the steel sheet will be described.
Al/N: satisfies the following formula (1)
－4.17×d+3.63≤Sol.Al/N≤－3.10×d+4.84 (1)
In the manufacturing method according to the present embodiment, it is important to control sol.al/N so as to satisfy the above formula (1) in the billet as a raw material in accordance with the final thickness of the produced unidirectional electromagnetic steel sheet.
In the manufacturing method according to the present embodiment, the present inventors manufactured electrical steel sheets having different final thicknesses for each sol.al/N by changing the sol.al/N of the billet as the starting material, and evaluated the magnetic flux density B8.
As a result, it was found that: in a region where sol.al/N satisfies the above formula (1), a magnetic flux density B8 of 1.930T or more can be obtained.
On the other hand, if Sol.Al/N exceeds "-3.10 × d + 4.84", a magnetic flux density B8 of 1.930T or more cannot be stably obtained. Therefore, Sol.Al/N is set to "-3.10 × d + 4.84" or less.
The reason is that: if the sol.al/N exceeds "-3.10 × d + 4.84", the primary recrystallization inhibitor becomes coarse and unevenly dispersed, the primary recrystallized structure after decarburization annealing becomes uneven, and good secondary recrystallization cannot be obtained on the entire steel sheet, and further, in decarburization annealing, in order to reduce the C content of the steel sheet to 25ppm or less, the annealing temperature needs to be increased, as a result, the primary recrystallization grain size increases, and a good driving force for secondary recrystallization cannot be ensured.
On the other hand, it is known that: if the ratio of Al/N is less than "-4.17 Xd + 3.63", a magnetic flux density B8 of 1.930T or more cannot be obtained. Therefore, Sol.Al/N is set to "-4.17 × d + 3.63" or more.
This is because, if sol.al/N is less than "-4.17 × d + 3.63", crystals of the secondary recrystallization having an orientation other than the gaussian orientation develop (the degree of aggregation of the gaussian orientation decreases), the magnetic flux density decreases, and the iron loss increases.
Next, process conditions of the production method according to the present embodiment will be described.
< Process conditions >
Steel billet
In the production method according to the present embodiment, a billet as a raw material can be obtained by melting in a converter, an electric furnace, or the like, subjecting the obtained molten steel to vacuum degassing treatment as necessary, and then performing continuous casting or ingot casting followed by cogging rolling. The billet is usually cast into a thin slab having a thickness of 150 to 350mm, preferably 220 to 280mm, but may be 30 to 70 mm. In the case of a thin slab, there is an advantage that rough machining to an intermediate thickness is not required in the production of a hot rolled steel sheet.
Hot rolling
Heating temperature: lower than 1250 deg.C
When the heating temperature of the slab subjected to hot rolling reaches 1250 ℃ or higher, the amount of molten oxide scale increases, and in the case of carrying out the production method according to the present embodiment, a dedicated heating furnace may be required in the production line.
Further, when the heating temperature reaches 1250 ℃ or higher, the crystal grain growth property in the primary recrystallization annealing is significantly deteriorated, and good secondary recrystallization cannot be achieved. This is due to the use of acid-soluble Al as an inhibitor in the present embodiment. After primary recrystallization in decarburization annealing described later, it is necessary to ensure the magnetic properties of the grain-oriented electrical steel sheet by setting the average grain size of the steel sheet to be in the range of 20 to 23 μm. The slab heating temperature before hot rolling has a large influence on the average crystal grain size after the primary recrystallization. When the slab heating temperature is 1250 ℃ or higher, fine AlN is precipitated in a large amount in the hot-rolled steel sheet after hot rolling, which hinders grain growth. On the other hand, when the slab heating temperature is set to less than 1250 ℃, the precipitated AlN is coarsened and the number thereof is reduced, and thus the refinement of crystal grains by the AlN can be suppressed.
When the heating temperature is 1250 ℃ or higher, MnS and/or MnSe are completely dissolved in a solid state and finely precipitated in the subsequent step. This also hinders grain growth as with AlN.
FIG. 1 shows an example of the structure of a grain-oriented electrical steel sheet obtained by a manufacturing method in which the slab heating temperature is 1250 ℃ and the decarburization annealing temperature is 800 ℃. FIG. 2 shows an example of the structure of a grain-oriented electrical steel sheet obtained by a manufacturing method in which the slab heating temperature is 1150 ℃ and the decarburization annealing temperature is 800 ℃. Other manufacturing conditions of the unidirectional electromagnetic steel sheet of fig. 1 and 2 are the same.
By comparing fig. 1 and fig. 2, it is found that: the metal structure of the steel sheet of fig. 1 having a slab heating temperature of 1250 deg.c is significantly smaller than that of the steel sheet of fig. 2 having a slab heating temperature of 1150 deg.c. It is estimated that the difference between the two is caused by the inhibition of grain growth by fine precipitates.
Even when the heating temperature of the billet exceeds 1250 ℃, the above-mentioned desired primary recrystallized grain size can be obtained by raising the decarburization annealing temperature (for example, by setting to over 1000 ℃). However, if the decarburization annealing temperature is increased, the primary recrystallization structure becomes uneven, and good secondary recrystallization cannot be obtained.
For the above reasons, the heating temperature of the billet is set to less than 1250 ℃, preferably 1200 ℃ or less, 1180 ℃ or less, or 1150 ℃ or less. The lower limit of the heating temperature of the slab is not particularly limited, and may be suitably selected according to the conditions for carrying out the usual hot rolling. For example, the billet may be heated to 1000 ℃ or higher, 1050 ℃ or higher, or 1100 ℃ or higher. The heated steel slab was subjected to hot rolling. The hot rolling may be carried out under known conditions, and the rolling conditions are not particularly limited.
Annealing of hot rolled sheet
The hot-rolled steel sheet is subjected to hot-rolled sheet annealing to make the uneven structure generated during hot rolling as uniform as possible. The annealing conditions are not particularly limited to specific conditions as long as they can make the generated uneven structure as uniform as possible.
For example, the non-uniform structure generated during hot rolling can be eliminated by heating a hot-rolled steel sheet to 1000 to 1150 ℃ (first stage temperature) to recrystallize it, and then annealing it at 850 to 1100 ℃ (second stage temperature) lower than the first stage temperature.
During this two-stage annealing, the first stage temperature exerts a large influence on the behavior of the inhibitor. If the first-stage temperature is too high, the inhibitor is finely precipitated in the subsequent step, and the decarburization annealing temperature for obtaining a desired primary recrystallized grain size is raised, so that the first-stage temperature is preferably 1150 ℃ or less.
If the first-stage temperature is too low, recrystallization is insufficient, and the nonuniform structure generated during hot rolling cannot be made uniform, so the first-stage temperature is preferably 1000 ℃ or higher, more preferably 1120 ℃ or higher.
Similarly to the first stage temperature, if the second stage temperature is too high, the inhibitor is finely precipitated in the subsequent step, and the decarburization annealing temperature for obtaining a desired primary recrystallized grain size is raised. Therefore, the second stage temperature is preferably 1100 ℃ or lower. If the second-stage temperature is too low, the γ phase is not generated and the hot-rolled structure cannot be made uniform, so the second-stage temperature is preferably 850 ℃ or higher, more preferably 900 ℃ or higher.
Pickling, cold rolling
Final plate thickness: 0.15 to 0.23mm
A hot-rolled steel sheet, from which the uneven structure during hot rolling is removed by hot-rolled sheet annealing, is subjected to acid pickling and then subjected to cold rolling, thereby forming a cold-rolled steel sheet having a final thickness of 0.15 to 0.23 mm. The cold rolling is preferably one cold rolling or two or more cold rolling with intermediate annealing interposed therebetween.
Cold rolling may be performed at normal temperature, or rolling may be performed at a temperature higher than normal temperature, for example, by raising the temperature of a steel sheet to about 200 ℃ (so-called warm rolling). The acid washing may be carried out under ordinary conditions.
If the final thickness of the cold-rolled steel sheet is less than 0.15mm, rolling is difficult, and secondary recrystallization tends to become unstable. Therefore, the final thickness of the cold-rolled steel sheet is set to 0.15mm or more, preferably 0.17mm or more.
On the other hand, if the final thickness of the cold-rolled steel sheet exceeds 0.23mm, the secondary recrystallization becomes too stable, and the difference in angle between the recrystallized grain orientation and the Gaussian orientation increases. Therefore, the final thickness of the cold-rolled steel sheet is set to 0.23mm or less. Preferably 0.21mm or less.
Decarburization annealing
In order to remove C contained in the cold-rolled steel sheet having a final thickness, decarburization annealing is performed on the cold-rolled steel sheet in a wet hydrogen atmosphere. The wet hydrogen atmosphere is, for example, a humidified gas having a dew point of 70 ℃, and is an atmosphere containing a trace amount of hydrogen as a gas species. More specifically, the annealing is performed in a humidified gas atmosphere having a dew point of 70 ℃ containing 10% of hydrogen, for example.
As described above, when the decarburization annealing temperature is too high, the primary recrystallization structure becomes uneven, and good secondary recrystallization cannot be obtained. Therefore, the decarburization annealing temperature is set to be lower than 1000 ℃. The lower limit of the decarburization annealing temperature can be selected as appropriate within the range in which the above-described effects can be obtained. For example, the decarburization annealing temperature may be set to 750 ℃ or more, 800 ℃ or more, or 850 ℃ or more. The lower limit is not necessarily set, but if the temperature is lower than 700 ℃, the grain growth and decarburization may not be sufficiently performed, so the decarburization annealing temperature is preferably 700 ℃ or higher.
The decarburization annealing is preferably performed by controlling the annealing atmosphere to a degree of oxidation at which no iron-based oxide is formed. For example, the oxidation degree of the annealing atmosphere is preferably 0.01 or more and less than 0.15. Degree of oxidation of PH2O/PH2The oxidation potential indicated.
If the degree of oxidation is less than 0.01, the decarburization rate becomes slow, and the productivity is lowered. On the other hand, if the degree of oxidation exceeds 0.15 or more, inclusions are formed under the surface of the product steel sheet, and the iron loss increases. The rate of temperature rise during heating is not particularly limited, and may be set to 50 ℃/sec or more, for example, from the viewpoint of productivity.
Nitriding treatment
A cold-rolled steel sheet subjected to decarburization annealing (hereinafter referred to as "steel sheet") is subjected to nitriding treatment so that the N content of the steel sheet becomes 40 to 1000 ppm. The nitriding treatment is not limited to a specific nitriding treatment. For example, the nitriding treatment may be performed in an atmosphere gas having nitriding ability such as ammonia.
If the N content of the steel sheet after nitriding treatment is less than 40ppm, AlN cannot be sufficiently precipitated and cannot sufficiently function as an inhibitor. In this case, since the secondary recrystallization cannot be sufficiently performed in the finish annealing, the N content of the steel sheet after the nitriding treatment is set to 40ppm or more, preferably 100ppm or more.
On the other hand, if the N content of the steel sheet after the nitriding treatment exceeds 1000ppm, AlN is present also after the end of secondary recrystallization in the finish annealing, which causes an increase in iron loss. Therefore, the N content of the steel sheet after nitriding treatment is set to 1000ppm or less, preferably 850ppm or less. Means for setting the N content of the steel sheet after nitriding to 40 to 1000ppm is not particularly limited. In general, the N content after the end of the nitriding treatment can be controlled by controlling the partial pressure of the nitrogen source (e.g., ammonia) in the nitriding atmosphere, the nitriding time, and the like.
Annealing the finished product
Annealing separating agent
And coating an annealing separating agent on the steel plate after the nitriding treatment, and carrying out finished product annealing. As the annealing separator, an annealing separator containing alumina, which is less reactive with silica, as a main component (containing 50 mass% or more of alumina) is used, and is preferably applied to the surface of the steel sheet by water slurry coating, electrostatic coating, or the like. By using the annealing separating agent, the surface of the finished product annealed steel plate can be processed into a smooth shape, and the iron loss is greatly reduced.
The steel sheet coated with the annealing separator is subjected to a finish annealing to perform secondary recrystallization, thereby gathering the crystal orientation in the {110} <001> orientation.
For example, the temperature of the final product is raised to 1100 to 1200 ℃ at a temperature raising rate of 5 to 15 ℃/hr in a nitrogen-containing annealing atmosphere, and the annealing atmosphere is switched to an atmosphere of 50 to 100% hydrogen at that temperature, and annealing with purification is performed for about 20 hours. However, the finish annealing conditions are not limited to these conditions, and can be selected as appropriate from known conditions.
Formation of insulating film
After the annealing of the product (after completion of the secondary recrystallization), the surface of the steel sheet is coated with an insulating film-forming coating liquid and sintered to form an insulating film, thereby producing a unidirectional electromagnetic steel sheet as a final product. The type of the insulating film is not limited to a specific one, and a known insulating film may be used.
For example, there is an insulating film formed by applying an aqueous coating liquid containing phosphate and colloidal silica. In the case of the insulating film, phosphates such as Ca, Al, Sr, and the like are preferable, and among them, aluminum phosphate salts are more preferable.
The colloidal silica is not limited to colloidal silica having specific properties. The particle size is not limited to a specific particle size, but is preferably 200nm or less (number average particle diameter). If the particle size exceeds 200nm, the coating solution may settle. On the other hand, colloidal silica having a particle size of less than 100nm is not problematic in dispersion, but the production cost is increased, which is not practical.
The coating liquid for forming an insulating film is applied to the surface of a steel sheet by a wet coating method such as a roll coater, and sintered in air at 800 to 900 ℃ for 10 to 60 seconds to form a tensile insulating film.
The grain-oriented electrical steel sheet may be subjected to domain refining treatment. It is preferable to form grooves on the surface of the steel sheet by the domain refining treatment to reduce the width of the magnetic domains, resulting in a reduction in the iron loss. Specific methods for the domain refining treatment are not particularly limited, but examples thereof include forming grooves by laser irradiation, electron beam irradiation, etching, gears, and the like.
Examples
Next, examples of the present invention will be described, but the conditions in the examples are one example of conditions adopted for confirming the feasibility and the effect of the present invention, and the present invention is not limited to the one example of conditions. The present invention can be applied to various conditions as long as the object of the present invention is achieved without departing from the gist of the present invention.
(example 1)
A steel slab having a composition shown in Table 1 (the remainder: Fe and impurities) was heated to 1150 ℃ and subjected to hot rolling to form a hot-rolled steel sheet having a thickness of 2.6mm, the first-stage temperature was set to 1100 ℃ and the second-stage temperature was set to 900 ℃, the hot-rolled steel sheet was subjected to hot-rolled sheet annealing and pickling, and cold-rolled once or multiple times with intermediate annealing interposed therebetween to form a cold-rolled steel sheet having a final thickness of 0.27mm, 0.23mm, 0.20mm, 0.18mm, 0.15mm, or 0.13 mm.
TABLE 1
Figure BDA0003162310920000151
Cold rolled steel sheets having a final thickness of 0.27mm, 0.23mm, 0.20mm, 0.18mm, 0.15mm or 0.13mm were subjected to decarburization annealing and nitriding treatment (annealing for increasing the nitrogen content of the steel sheet). Specifically, decarburization annealing was performed at a temperature increase rate of 100 ℃/sec with the degree of oxidation of the atmosphere set to 0.12. The soaking temperature in the decarburization annealing is shown in table 2. Then, the cold-rolled steel sheet was subjected to nitriding treatment so as to attain the nitrogen content shown in table 2.
The surface of the steel sheet subjected to decarburization annealing and nitriding treatment was coated with an annealing separator containing alumina as a main component, and the steel sheet was heated at a temperature rise rate of 15 ℃/hr to carry out finish annealing at 1200 ℃. An aqueous coating solution containing phosphate and colloidal silica was applied and fired in air at 800 ℃ for 60 seconds to form an insulating film (tensile insulating film).
Whether or not the steel sheet before the nitriding treatment satisfies the above formula (1) was confirmed, and the nitrogen content and carbon content of the steel sheet after the decarburization and nitriding treatment were measured.
The magnetic flux density B8(T) and the iron loss W of the steel sheet after the annealing of the finished product and the formation of the insulating film and after the magnetic domain control were measured17/50. Due to iron loss W17/50Since the thicknesses vary greatly, examples in which the thicknesses are 0.27mm, 0.23mm, 0.20mm, 0.18mm, 0.15mm and 0.13mm and the iron losses are 0.75W/kg or less, 0.65W/kg or less, 0.62W/kg or less, 0.55W/kg or less, 0.50W/kg or less and 0.45W/kg, respectively, are regarded as examples in which good magnetic properties are obtained. As long as the magnetic flux density B8(T) is 1.930T or more, it is considered that a good magnetic characteristic is obtained.
TABLE 2
Figure BDA0003162310920000171
In the invention examples satisfying the conditions of the present invention, the carbon content (C content) after the decarburization nitriding treatment was reduced to 25ppm or less, and the magnetic flux density B8 and the iron loss W were used17/50The magnetic properties shown are good. In contrast, in comparative examples other than the conditions of the present invention, the amount of carbon was large, and the iron loss W was caused17/50Poor secondary recrystallization and low magnetic flux density, resulting in low iron loss W17/50Is an inferior bit.
(example 2)
Slabs having the composition shown in table 1 were subjected to hot rolling at various slab heating temperatures shown in table 3 to form hot-rolled steel sheets having a thickness of 2.6mm, the first-stage temperature was set to 1100 ℃ and the second-stage temperature was set to 900 ℃, the hot-rolled steel sheets were subjected to hot-rolled sheet annealing and pickling, and then subjected to one cold rolling or multiple cold rolling with intermediate annealing, thereby forming cold-rolled steel sheets having a final thickness of 0.23mm or 0.20 mm.
A cold rolled steel sheet having a final thickness of 0.23mm or 0.20mm is subjected to decarburization annealing and nitriding treatment (annealing for increasing the nitrogen content of the steel sheet). The decarburization annealing was performed at a temperature rise rate of 80 ℃/sec with the degree of oxidation of the atmosphere set to 0.12. The soaking temperature in the decarburization annealing is shown in table 3. Then, the cold-rolled steel sheets were subjected to nitriding treatment so as to attain the nitrogen amount (N content) described in table 3. The surface of the steel sheet subjected to decarburization annealing and nitriding is coated with an annealing separator containing alumina as a main component, and the steel sheet is heated at a temperature rise rate of 15 ℃/hr to perform finish annealing at 1200 ℃. Further, an aqueous coating solution containing phosphate and colloidal silica was applied and fired in air at a temperature of 800 ℃ for 60 seconds to form a tensile insulating film.
Whether or not the steel sheet before the nitriding treatment satisfies the above formula (1) was confirmed, and the nitrogen content and carbon content of the steel sheet after the decarburization and nitriding treatment were measured. Further, the magnetic flux density B8(T) and the iron loss W of the steel sheet after the finish annealing and the formation of the insulating film and after the magnetic domain control by laser irradiation were measured17/50. The evaluation criteria were the same as in example 1. The results are shown in Table 3.
Figure BDA0003162310920000191
In the example of the present invention in which the slab heating temperature is less than 1250 ℃, the magnetic flux density B8 and the iron loss W are used17/50The magnetic properties shown are good, while the comparative examples other than the slab heating condition of the present invention have poor secondary recrystallization and low magnetic flux density,iron loss W17/50Is an inferior bit.
(example 3)
A steel slab having a composition shown in Table 1 was subjected to hot rolling at 1150 ℃ to form a hot-rolled steel sheet having a thickness of 2.6mm, the first-stage temperature was set to 1100 ℃ and the second-stage temperature was set to 900 ℃, the hot-rolled steel sheet was subjected to hot-rolled sheet annealing, and then the hot-rolled steel sheet was subjected to annealing at 900 ℃ and then to pickling, and subjected to cold rolling once or multiple times with intermediate annealing interposed therebetween to form a cold-rolled steel sheet having a final thickness of 0.23mm or 0.20 mm.
A cold rolled steel sheet having a final thickness of 0.23mm or 0.20mm is subjected to decarburization annealing and nitriding treatment (annealing for increasing the nitrogen content of the steel sheet). The decarburization annealing was performed at a temperature rise rate of 100 ℃/sec with the degree of oxidation of the atmosphere set to 0.12. The soaking temperature in the decarburization annealing is shown in table 4. Then, the cold-rolled steel sheets were subjected to nitriding treatment so as to attain the nitrogen content shown in table 4. The surface of the steel sheet subjected to decarburization annealing and nitriding treatment was coated with an annealing separator containing alumina as a main component, and finish annealing was performed at 1200 ℃ at a temperature rise rate of 15 ℃/hr. Further, an aqueous coating solution containing phosphate and colloidal silica was applied and fired in air at a temperature of 800 ℃ for 60 seconds to form a tensile insulating film.
Whether or not the steel sheet before the nitriding treatment satisfies the above formula (1) was confirmed, and the nitrogen content and carbon content of the steel sheet after the decarburization and nitriding treatment were measured. Further, the magnetic flux density B8(T) and the iron loss W of the steel sheet after the finish annealing and the formation of the insulating film and after the magnetic domain control by laser irradiation were measured17/50. The evaluation criteria were the same as in example 1. The results are shown in Table 4.
Figure BDA0003162310920000211
In the inventive example in which the nitrogen content after decarburization/nitridation is in the range of 40 to 1000ppm, the magnetic flux density and the iron loss W17/50On the other hand, in comparative examples other than the nitrogen amount of the present invention, the secondary recrystallization became poorEven after the annealing of the final product, residual nitrides precipitated, and the magnetic flux density B8(T) and the iron loss W17/50Is an inferior bit.
(example 4)
A steel slab having a composition shown in Table 1 was subjected to hot rolling at 1150 ℃ to form a hot-rolled steel sheet having a thickness of 2.6mm, the first stage temperature was set to 1100 ℃ and the second stage temperature was set to 900 ℃, the hot-rolled steel sheet was subjected to hot-rolled sheet annealing, then the hot-rolled steel sheet was subjected to annealing at 900 ℃ and then to pickling, and then subjected to cold rolling once or multiple times with intermediate annealing interposed therebetween to form a cold-rolled steel sheet having a final thickness of 0.23mm or 0.20 mm.
A cold rolled steel sheet having a final thickness of 0.23mm or 0.20mm is subjected to decarburization annealing and nitriding treatment (annealing for increasing the nitrogen content of the steel sheet). The decarburization annealing was performed at a temperature rise rate of 100 ℃/sec with the degree of oxidation of the atmosphere set to 0.12. The soaking temperature in the decarburization annealing is shown in table 5. Then, the cold-rolled steel sheets were subjected to nitriding treatment so as to attain the nitrogen content shown in table 5. The surface of the decarburized and nitrided steel sheet was coated with an annealing separator containing alumina as a main component, and the steel sheet was heated at a temperature rise rate of 15 ℃/hr to carry out finish annealing at 1200 ℃. Further, an aqueous coating solution containing phosphate and colloidal silica was applied and fired in air at a temperature of 800 ℃ for 60 seconds to form a tensile insulating film.
Whether or not the steel sheet before the nitriding treatment satisfies the above formula (1) was confirmed, and the nitrogen content and carbon content of the steel sheet after the decarburization and nitriding treatment were measured. The magnetic flux density B8(T) and the iron loss W of the steel sheet after the finish annealing and the application of the insulating film and after the magnetic domain control by laser irradiation were measured17/50. The evaluation criteria were the same as in example 1. The results are shown in Table 5.
Figure BDA0003162310920000231
In the inventive example in which the decarburization annealing temperature is less than 1000 ℃, the magnetic flux density B8 and the iron loss W were used17/50Exhibits good magnetic properties as shown inWhen the decarburization annealing temperature is 1000 ℃ or higher and is out of the range of the present invention, the magnetic flux density B8 and the iron loss W17/50Relative to the invention example is the inferior bit.
Industrial applicability
As described above, according to the present invention, it is possible to stably provide a grain-oriented electrical steel sheet having a sheet thickness of 0.15 to 0.23mm and excellent magnetic properties. Therefore, the present invention has high applicability in the manufacturing and application industries of electrical steel sheets.

Claims (2)

1. A method for manufacturing a grain-oriented electrical steel sheet, comprising:
heating a steel slab to less than 1250 ℃ and subjecting to hot rolling to form a hot-rolled steel sheet, the steel slab containing, in mass%, C: 0.100% or less, Si: 0.80 to 7.00%, Mn: 0.05-1.00%, Sol.Al: 0.0100-0.0700%, N: 0.0040-0.0120%, Seq ═ S +0.406 × Se: 0.0030-0.0150%, Cr: 0-0.30%, Cu: 0-0.40%, Sn: 0-0.30%, Sb: 0-0.30%, P: 0-0.50%, B: 0-0.0080%, Bi: 0-0.0100%, Ni: 0 to 1.00%, the remainder comprising Fe and impurities,
subjecting the hot rolled steel sheet to hot-rolled sheet annealing,
pickling the hot rolled steel sheet after the annealing of the hot rolled steel sheet,
subjecting the hot-rolled steel sheet after pickling to cold rolling to form a cold-rolled steel sheet having a final thickness d of 0.15 to 0.23mm,
the cold-rolled steel sheet is subjected to decarburization nitriding treatment including decarburization annealing and nitriding treatment,
performing finish annealing on the cold-rolled steel sheet after the decarburized and nitrided process,
coating the finished annealed cold-rolled steel sheet with an insulating coating film-forming coating liquid and sintering the coated cold-rolled steel sheet;
wherein the slab has a Sol.Al/N ratio of Sol.Al to N by mass and a final plate thickness d satisfying the following formula (1),
the N content of the cold-rolled steel sheet after the decarburization and nitridation treatment is 40 to 1000ppm,
the decarburization annealing temperature in the decarburization annealing is lower than 1000 ℃,
－4.17×d+3.63≤Sol.Al/N≤－3.10×d+4.84 (1)。
2. the method of manufacturing a grain-oriented electrical steel sheet according to claim 1, wherein the steel slab contains 1 or two or more of the following elements in mass%:
Cr：0.02～0.30％、
Cu：0.10～0.40％、
Sn：0.02～0.30％、
Sb：0.02～0.30％、
P：0.02～0.50％、
B：0.0010～0.0080％、
Bi：0.0005～0.0100％、
Ni：0.02～1.00％。
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